黔产天麻的化学成分

从黔产天麻（Ｇａｓｔｒｏｄｉａ ｅｌａｔａ Ｂｌ．）中分离得到１个新的含氮化合物,命名为天麻羟胺（ｇａｓｔｒｏｄａｍｉｎｅ,Ⅰ）,经波谱分析,确定其结构为双－（对羟苄基）羟胺。除β－谷甾醇和胡萝卜甙外,同时还分离鉴定了３个已知化合的：Ｌ－焦谷氨酸（Ⅱ）、柠檬酸单甲酯（Ⅲ）、柠檬酸双甲酯（Ⅳ）,其中化合物Ⅱ和Ⅳ为首次报道从天麻中得到的。     

两种水溶性抗菌活性物质的分离提取

对水溶性、不解离的极性物质分离时,一般采用吸附层析和凝胶层析等途径。实验通过硅胶柱层析、葡聚糖凝胶柱层析以及硅胶ＧＦ２５４制备型薄板层析,从发酵液样品中分离出两种有抗菌活性的纯物质。薄层层析的展开剂为二氯甲烷－四氢呋喃－甲醇－水（２５：３０：２）,分离出的组分中Ｒｆ＝０．７和Ｒｆ＝０．８两种物质有抗菌活性。硅胶柱层析洗脱过程为梯度洗脱,先用１５０ｍｌ上述展开剂洗脱,再用二氯甲烷－甲醇（２０：８０）     

倒心盾翅藤的化学成分研究

从药用植物倒心盾翅藤（Aspidopterys obcordata Hemsl.）中首次分离得到５个化合物,通过波谱分析分别鉴定为木栓酮（１）、无羁萜－３β－醇（２）、二二烷酸甲酯（３）、１０－二九烷醇（４）、豆甾醇（５）和daphnetin-8-glucopyranoside(6)。     

螺旋藻β—胡萝卜素的分离提纯研究

研究了螺旋藻β－胡萝卡素的提取和分离纯化方法。用丙酮－甲醇（７：２,ｖ：ｖ）可快速彻底地将螺旋藻的色素抽提出来,再用乙醚和５％ＮａＣｌ水溶液分离纯化后,经紫外可见分光光度计扫描分析可知产品为纯度较高的β－胡萝卜素,β－胡萝卜素产量为６．７５ｍｇ／ｇ干螺旋藻,提取率为７５％。     

人胎肝中低分子抑瘤物的分离纯化、结构鉴定及其对肿瘤细胞生长的选择性抑制

在胎儿组织中存在一类低分子肿瘤抑制物,胎肝细胞的甲醇－丙酮提取物中保留有大部分抑瘤活性,用体外液体培养条件下对人急性粒系白血病细胞系（HL－60）的抑制作用为指标,跟踪指导分离过程,提取物经反相C18中压液相色谱,Sephadex LH-20凝胶色谱及氨基键合相高效液相色谱分离得到一纯活性物质。经NMR和MS鉴定为7－酮基胆固醇（7－ketocholesterol,7-KC)。体外琼脂培养条件下7－KC对小鼠WEHI－3和S－180细胞较对正常小鼠骨髓粒－巨噬系祖细胞有更强的抑制增殖及集落生成作用,7－KC对HL－60细胞增殖较对正常人骨髓CFU－GM有更强的抑制作用。     

鸡屎藤挥发油化学成分的研究

利用气相色谱－质谱联用（ＧＣ／ＭＳ）技术对鸡屎藤挥发油化学成分进行分析研究,初步鉴定了３１种成分,它们占挥发油总量的７７．１６％,其中含量友上的有乙氧戊烷、乙酸异戊酯、苯甲醛、己酸乙酯、甲酸苯甲酯、乙酸苯甲酯、乙酸－２－苯乙酯、５,６,７,７ａ－四氢－４,４,７ａ－三甲基－２（４Ｈ）－苯并呋喃酮、十五碳酸乙酯、十六碳酸和癸酸异戊酯等１１种成分。     

人胎肝中低分子抑瘤物的分离纯化、结构鉴定及其对肿瘤细胞生长的选择性抑制作用

在胎儿组织中存在一类低分子肿瘤抑制物。胎肝细胞的甲醇－丙酮提取物中保留有大部分抑瘤活性。用体外液体培养条件下对人急性粒系白血病细胞系（ＨＬ－６０）的抑制作用为指标,跟踪指导分离过程。提取物经反相Ｃ１８中压液相色谱、ＳｅｐｈａｄｅｘＬＨ－２０凝胶色谱及氨基键合相高效液相色谱分离得到一纯活性物质,经ＮＭＲ和ＭＳ鉴定为７－酮基胆固醇（７－ｋｅｔｏｃｂｌｅｓｔｅｒｏｌ,７－ＫＣ）。体外琼脂培养条件下７－ＫＣ对小鼠ＷＥＨ１－３和Ｓ－１８０细胞较对正常小鼠骨髓粒一巨噬系祖细胞有更强的抑制增殖及集落生成作用。７－ＫＣ对ＨＬ－６０细胞增殖较对正常人骨髓ＣＦＵ－ＧＭ有更强的抑制作用。     

南瓜籽抗前列腺增生化学成分研究

本文研究了南瓜籽抗前列腺增生活性及功效成分。南瓜籽乙醇回流提取,经石油醚萃取,硅胶柱、ODS反向柱层析柱分离,用核磁共振方法鉴定结构。结果表明:南瓜籽醇提石油醚萃取相经硅胶柱层析氯仿∶甲醇(8∶2、7∶3)梯度洗脱物对小鼠前列腺增生活性的抑制效果最明显,再经ODS柱分离,得到了三个单体化合物,分别为3-甲酸-1,4-环己二烯-2-十一烷酸甲酯(1),3-甲酸-1,4-环己二烯-2-十一烯酸甲酯(2),2-十一烯酸甲酯-3-十一烷酸-环己-1,4-二烯酯(3)。化合物1~3为首次从南瓜籽中分离得到的酯类物质。     

灯盏花中的糖苷

从灯盏花（Erigeron breviscapus (Vant.) Hand.-Mazz.) 全株的乙醇提取物的正丁醇部分分得10个化合物,通过波谱方法鉴定为erigeside I(1)、γ－吡喃酮－3－O－β－D－[6′－（4″－羟基－3″,5″－二甲氧基苯甲酰）-]-吡喃葡萄糖苷（erigeside D,2)、erigeside A(3)、erigeside B(4)、erigeside Ⅱ(5)、7-O-β-D-吡喃葡萄糖－6－甲氧基香豆素（6）、icariside B2(7)、blumenol C葡萄糖苷（8）、（＋）－丁香树酯醇O－β－D－吡喃葡萄糖苷（9）和野黄芩苷甲酯（10）。用X射线单晶衍射方法确定了化合物7的绝对构型。2是一个新化合物,7、8和9首次从该属植物分离得到,6首次从该种植物分离得到。     

长臂生物素对硝基苯酯的合成

以羰基二咪唑为催化剂,生物素与6－氨基己酸甲酯反应生成生物素－6－氨基己酸甲酯,该化合物通过酸碱萃取与原料分离,皂化后生成生物素氨基己酸．生物素氨基己酸在吡啶存在下与三氟乙酸对硝基苯酯进行转酯反应即得生物素对硝基苯酯．最后经光谱、色谱及核酸杂交证实了长臂生物素对硝基苯酯的化学结构和生物学活性．     

Synthesis and characterization of vegetable oil derived esters: evaluation for their diesel additive properties

Trans-esterification of four vegetable oils; canola oil, greenseed canola oil from heat-damaged seeds, processed waste fryer grease and unprocessed waste fryer grease, was carried out using methanol, and KOH as catalyst. The methyl esters of the corresponding oils were separated from the crude glycerol, purified, and characterized by various methods to evaluate their densities, viscosities, iodine values, acid numbers, cloud points, pour points and gross heat of combustion, fatty acid and lipid compositions, lubricity properties, and thermal properties. The fatty acid composition suggests that 80-85% of the ester was from unsaturated acids. Substantial decrease in density and viscosity of the methyl esters compared to their corresponding oils suggested that the oils were in their mono or di glyceride form. The lubricity of the methyl esters, when blended at 1 vol% treat rate with ISOPAR M reference fuel, showed that the canola methyl ester enhanced the fuel's lubricity number. From the analyses performed, it was determined that the ester with the most potential for being an additive or a substitute for diesel fuel is the canola methyl ester, whose physical and chemical characteristics are similar to diesel fuel.     

The effect of the acidity of rapeseed oil on its transesterification

The aim of this work is to study the transesterification of vegetable oil with a high acid number at unchanged reaction conditions. Rapeseed oil was used as the raw material and its acid number was changed by the addition of oleic acid (from 0.89 to 12.25 mg KOH/g). Methanol was used for transesterification (molar ratio of oil to methanol 1:6) and potassium hydroxide was used as a catalyst. After the reaction time, the residue of the catalyst was neutralised by gaseous carbon dioxide and the methanol excess was removed. After the separation of two phases, each of them was analyzed (in the ester phase: yield, content of methyl ester and acid number; in the glycerol phase: yield, density, viscosity, content of glycerol, soaps, methyl ester, potassium carbonate and hydrogen carbonate). The obtained data was compared with theoretical material balances and the effect on the saponification of oil was discussed. The results show that the yield of methyl ester (biodiesel) is significantly affected by a higher acid number, as well as enhanced soap formation. On the other hand, the conversion of the oil and acid number of the ester phase remain at constant values in studied borders.     

Transesterification of canola oil in mixed methanol/ethanol system and use of esters as lubricity additive

Transesterification of canola oil was carried out with methanol, ethanol, and various mixtures of methanol/ethanol, keeping the molar ratio of oil to alcohol 1:6 and using KOH as a catalyst. Mixtures of alcohol increased the rate of transesterification reaction and produced methyl as well as ethyl esters. The increased rate was result of better solubility of oil in reaction mixture due to better solvent properties of ethanol than methanol and equilibrium due to methanol. With 3:3 molar ratio of methanol to ethanol {MEE (3:3)} the amount of ethyl ester formed was 50% that of methyl ester. Properties (acid value, viscosity, density) of all esters including mixed esters were within the limits of ASTM standards. Lubricities of these esters are in the order: ethyl ester>methyl ethyl ester>methyl ester.     

Divergent effects of eicosapentaenoic and docosahexaenoic acid ethyl esters, and fish oil on hepatic fatty acid oxidation in the rat

The physiological activity of fish oil, and ethyl esters of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) affecting hepatic fatty acid oxidation was compared in rats. Five groups of rats were fed various experimental diets for 15 days. A group fed a diet containing 9.4% palm oil almost devoid of n-3 fatty acids served as a control. The test diets contained 4% n-3 fatty acids mainly as EPA and DHA in the form of triacylglycerol (9.4% fish oil) or ethyl esters (diets containing 4% EPA ethyl ester, 4% DHA ethyl ester, and 1% EPA plus 3% DHA ethyl esters). The lipid content of diets containing EPA and DHA ethyl esters was adjusted to 9.4% by adding palm oil. The fish oil diet and ethyl ester diets, compared to the control diet containing 9.4% palm oil, increased activity and mRNA levels of hepatic mitochondrial and peroxisomal fatty acid oxidation enzymes, though not 3-hydroxyacyl-CoA dehydrogenase activity. The extent of the increase was, however, much greater with the fish oil than with EPA and DHA ethyl esters. EPA and DHA ethyl esters, compared to the control diet, increased 3-hydroxyacyl-CoA dehydrogenase activity, but fish oil strongly reduced it. It is apparent that EPA and DHA in the form of ethyl esters cannot mimic the physiological activity of fish oil at least in affecting hepatic fatty acid oxidation in rat.     

Optimization of alkali-catalyzed transesterification of Pongamia pinnata oil for production of biodiesel

Studies were carried out on transesterification of Karanja oil with methanol for the production of biodiesel. The reaction parameters such as catalyst concentration, alcohol/oil molar ratio, temperature, and rate of mixing were optimized for production of Karanja oil methyl ester (KOME). The fatty acid methyl esters content in the reaction mixture were quantified by HPLC and 1H NMR method. The yield of methyl esters from Karanja oil under the optimal condition was 97-98%.     

Lipase specificity towards eicosapentaenoic acid and docosahexaenoic acid depends on substrate structure

The fatty acid specificity of five lipases towards eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) was evaluated in the hydrolysis of fish oil, squid oil and a model system. The model system contained methyl esters of EPA, DHA and palmitic acid. All the investigated lipases discriminated against both EPA and DHA more in the model system than in the natural oils. Thus both EPA and DHA were more easily hydrolysed from a glyceride than from a methyl ester. In the model system, the lipase from Candida rugosa showed the highest discrimination against DHA, while the lipases from Pseudomonas fluorescens and Pseudomonas cepacia discriminated against EPA the most. In a glyceride, the fatty acid specificity of lipases towards EPA and DHA was affected by the positional distribution of the fatty acids and the glyceride structure due to the regiospecificity and triglyceride specificity of the lipase. In the oils, the Pseudomonas lipases also discriminated against EPA the most, while DHA was initially discriminated the most by the lipase from Thermomyces lanuginosus. However, after longer reaction times the enrichment of DHA in the glyceride fraction of the oils was greatest for the lipase from C. rugosa.     

Selection of lipase producing yeasts for methanol-tolerant biocatalyst as whole cell application for palm-oil transesterification

Methanol-tolerant lipase producing yeast was successfully isolated and selected thorough ecological screening using palm oil-rhodamine B agar as one step-approach. All 49 lipase-producing yeasts exhibited the ability to catalyze esterification reaction of oleic acid and methanol at 3 molar equivalents. However, only 16 isolates catalyzed transesterification reaction of refined palm oil and methanol. Rhodotorula mucilagenosa P11I89 isolated from oil contaminated soil showed the strongest hydrolytic lipase activity of 1.2U/ml against palm oil. The production of oleic methyl ester and fatty acid methyl ester (FAME) of 64.123 and 51.260% was obtained from esterification and transesterification reaction catalyzed by whole cell of R. mucilagenosa P11I89 in the presence of methanol at 3 molar equivalents against the substrates, respectively. FAME content increased dramatically to 83.29% when 6 molar equivalents of methanol were added. Application of the methanol-tolerant-lipase producing yeast as a whole cell biocatalyst was effectively resolved major technical obstacles in term of enzyme stability and high cost of lipase, leading to the feasibility of green biodiesel industrialization.     

Preparation of biodiesel from crude oil of Pongamia pinnata

Biodiesel was prepared from the non-edible oil of Pongamia pinnata by transesterification of the crude oil with methanol in the presence of KOH as catalyst. A maximum conversion of 92% (oil to ester) was achieved using a 1:10 molar ratio of oil to methanol at 60 degrees C. Tetrahydrofuran (THF), when used as a co-solvent increased the conversion to 95%. Solid acid catalysts viz. Hbeta-Zeolite, Montmorillonite K-10 and ZnO were also used for this transesterification. Important fuel properties of methyl esters of Pongamia oil (Biodiesel) compare well (Viscosity = 4.8 Cst @ 40 degrees C and Flash point = 150 degrees C) with ASTM and German biodiesel standards.     

Optimisation of integrated biodiesel production. Part II: a study of the material balance

A study was made of the material balance for the fatty acid methyl ester (biodiesel) synthesis from sunflower oil using potassium hydroxide as the catalyst. A factorial design of experiments and a central composite design have been used to evaluate the influence of operating conditions on the process material balance. The responses chosen were the biodiesel yield and the yield losses due to triglyceride saponification and methyl ester dissolution in glycerol, while the variables studied were temperature, initial catalyst concentration and the methanol:vegetable oil molar ratio. The biodiesel yield increased and therefore the yield losses decreased by decreasing catalyst concentration and temperature. However, the methanol:sunflower oil molar ratio did not affect the material balance variables significantly. Second-order models were obtained to predict the biodiesel yield and both yield losses. Within the experimental range studied, these models largely matched the results from the experiments.     

Biodiesel production from high acid value waste frying oil catalyzed by superacid heteropolyacid

Transesterification of waste cooking oil with high acid value and high water contents using heteropolyacid H3PW12O40 x 6H2O (PW12) as catalyst was investigated. The hexahydrate form of PW(12) was found to be the most promising catalyst which exhibited highest ester yield 87% for transesterification of waste cooking oil and ester yield 97% for esterification of long-chain palmitic acid, respectively. The PW12 acid catalyst shows higher activity under the optimized reaction conditions compared with conventional homogeneous catalyst sulfuric acid, and can easily be separated from the products by distillation of the excess methanol and can be reused more times. The most important feature of this catalyst is that the catalytic activity is not affected by the content of free fatty acids (FFAs) and the content of water in the waste cooking oil and the transesterification can occur at a lower temperature (65 degrees C), a lower methanol oil ratio (70:1) and be finished within a shorter time. The results illustrate that PW12 acid is an excellent water-tolerant and environmentally benign acid catalyst for production of biodiesel from waste cooking oil.